高效液相色谱法测定蔗糖-6-乙酯  

Determination of sucrose-6-acetate by high performance liquid chromatography

作　　者：杨欣宜 郭辉[1] 陈云菲 钱俊青[1] 庄勇 YANG Xinyi;GUO Hui;CHEN Yunfei;QIAN Junqing;ZHUANG Yong(Zhejiang University of Technology,Hangzhou 310000,China;Nantong Changhai Food Additive Co.,Ltd.,Nantong 226000,China)

机构地区：[1]浙江工业大学,浙江杭州310000 [2]南通市常海食品添加剂有限公司,江苏南通226000

出　　处：《食品与发酵工业》2019年第22期240-245,共6页Food and Fermentation Industries

基　　金：“十三五”国家重点研发计划课题(2016YFD0400803)

摘　　要：蔗糖-6-乙酯是制备三氯蔗糖的关键中间体,建立一种准确、快速的分析方法测定蔗糖-6-乙酯是这种甜味剂生产质控关键。采用高效液相色谱-蒸发光散射法(high performance liquid chromatography-evaporative light scattering detector,HPLC-ELSD)检测蔗糖-6-乙酯,使用ZORBAX SB-Aq色谱柱,以甲醇水溶液(V(甲醇)∶V(水)=5∶90)为流动相,流速为0.8 m L/min,蒸发光漂移管温度为85℃,氮气流速为1.5 L/min。同时对内标法及外标法检测蔗糖-6-乙酯进行了方法学验证。实验表明,2种方法的线性范围均为1.10~11.03 g/L,线性相关系数均在0.99以上,其中外标法的RSD值均小于3.0%,而内标法的RSD值均小于2.0%,并且内标法的检出限和定量限均低于外标法,分别为31.04及103.46μg/m L。2种方法均能检测蔗糖-6-乙酯,其中内标法略优于外标法。该研究建立的方法可用于蔗糖-6-乙酯的含量检测,并为蔗糖酯的检测分析提供了参考。Sucrose-6-acetate is a key intermediate for sucralose preparation.Establishing an accurate and rapid analytical method for the determination of sucrose-6-acetate is essential for the quality control in sucralose production.Sucrose-6-acetate was detected by high performance liquid chromatography-evaporative light scattering(HPLCELSD).The analytical column was ZORBAX SB-Aq column with methanol/water(5∶90,V/V)as the mobile phase at a flow rate of 0.8 m L/min.The evaporative light drift tube temperature was 85℃and the nitrogen flow rate was1.5 L/min.The method was verified by internal standard method and external standard method for the detection of sucrose-6-acetate.The linear range of both methods was 1.10-11.03 mg/m L,with the linear correlation coefficient of above 0.99.The RSD value of the external standard method was less than 3.0%,and that of the internal standard method was less than 2.0%.In addition,the detection limit and quantification limit of the internal standard method were lower than the external standard method,which were 31.04 mg/m L and 103.46 mg/m L,respectively.Both methods could detect sucrose-6-acetate,and the internal standard method was slightly better than the external standard method.The method established in this study can be used for the determination of sucrose-6-acetate,which provides a reference for the detection and analysis of sucrose esters.

关 键 词：蔗糖-6-乙酯 高效液相色谱-蒸发光散射 内标法 外标法 方法学验证 

分 类 号：R28[医药卫生—中药学]